ASTM_D_6806_-_02_2012.pdf

Designation:D680602(Reapproved 2012)Standard Practice forAnalysis of Halogenated Organic Solvents and TheirAdmixtures by Gas Chromatography1This standard is issued under the fixed designation D6806;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This practice covers the determination of impurities,stabilizers and assay of halogenated organic solvents and theiradmixtures by gas chromatography.1.2 It is not the intent of this practice to provide a specificmethod of gas chromatography.The intent of this practice is todefine what is required for a user to demonstrate that a methodto be used is valid.The reason for this approach,as opposed tostating a method,is that gas chromatography is such a dynamicfield that methods are often obsolete by the time they arevalidated.The use of this practice allows the user to use mosteffective technology and demonstrate that the method in usecomplies with a standard practice and is valid for the analysisof halogenated organic solvents and their admixtures.1.3 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)33.Terminology3.1 Purity and assay are used interchangeably in this stan-dard.3.1.1 Purity or assay are defined as 100 sum(impurities+stabilizer)when impurities and stabilizers are expressed in%;3.1.2 Or 100 sum(impurities+stabilizer)/10 000 whenimpurities are expressed in ppm.3.2 Accuracy is defined per A2.2.1 of Practice E180 or theagreement between an experimentally determined value andthe accepted reference value.3.3 Precision is defined per A2.1.7 of Practice E180 or thedegree of agreement of repeated measurements of the sameproperty.It is generally expressed in standard deviations orpercent relative standard deviation(s/X)100,also known ascoefficient of variation.4.Summary of Practice4.1 This practice will define the requirements for a gaschromatographic(GC)method to be valid for the determina-tion of impurities,stabilizers and assay of halogenated organicsolvents and their admixtures.5.Method Requirements5.1 The GC method must give adequate separation of theimpurities and stabilizers common to the product in question sothat the instrument response(area counts,millivolts,etc.)to theindividual impurities or stabilizers can be measured withadequate precision and accuracy as defined in Section 6.Process knowledge from the supplier or manufacturer of theproduct is a resource of information as to what those impuritiesand stabilizers are.GC-Mass Spectrometry(GC-MS)is an-other resource to initially determine what components arepresent to be measured.See Table 1 for a list of possibleimpurities and stabilizers for each product.5.2 Non polar capillary columns of about 0.32 mm by 30 mgenerally work well.Table 2 provides a list of columns thatmay prove suitable for the analysis of the halogenated organicproducts.5.3 Instrument ConditionsThe following GC conditionsare often appropriate for the analysis of halogenated organicproducts and their admixtures though actual conditions shouldbe optimized for the analysis being performed.5.4 The separation is determined to be adequate by prepar-ing standards of known amounts of the impurities and stabi-lizers in concentrations near enough to the expected concen-trations in the sample for the instrument response to be linear1This practice is under the jurisdiction of ASTM Committee D26 on Haloge-nated Organic Solvents and Fire Extinguishing Agents and is the direct responsi-bility of Subcommittee D26.04 on Test Methods.Current edition approved March 1,2012.Published June 2012.Originallyapproved in 2002.Last previous edition approved in 2007 as D6806-02(2007).DOI:10.1520/D6806-02R12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 over the concentration range of interest.Repeated injections(minimum of three)of this standard are made and the accuracyand precision of the method for the individual impurities andstabilizers are determined.5.5 Response to components must not be out of range of thedetector and should be su